2-Aminopyridine → HCID 13633211、化合物

HRID 2118495ノート

反応式

HRID 2118495 の反応式
C(N1C=CN=C1)(N1C=CN=C1)=O.[N+:13]1([O-:22])[C:14]([C:19]([OH:21])=O)=[CH:15][CH:16]=[CH:17][CH:18]=1.[NH2:23][C:24]1[CH:29]=[CH:28][CH:27]=[CH:26][N:25]=1>CN(C)C=O>[N:25]1[CH:26]=[CH:27][CH:28]=[CH:29][C:24]=1[NH:23][C:19]([C:14]1[N+:13]([O-:22])=[CH:18][CH:17]=[CH:16][CH:15]=1)=[O:21]

参加物

5

反応物 3

HCID 104392-AminopyridineHCID 682631,1'-CarbonyldiimidazoleHCID 69986Pyridine-2-carboxylic acid 1-oxide

生成物 1

HCID 13633211HCID 13633211、化合物収率 0.1%

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

1,1'-Carbonyldiimidazole (4.254 g, 26.2 mol) was added to a solution of picolinic acid N-oxide (3.318g, 23.9 mol) in dry dimethylformamide (50 ml). After 4 hours, 2-aminopyridine (2.466 g, 26.2 mol) was added. After 1 hour, the solution was warmed to 100° for 80 minutes and cooled to room temperature. After 18 hours the solution was subjected to evaporation in vacuo to give an oil which slowly crystallised. The solid was recrystallised from EtOH to give the title compound (3.775 g) as needles, m.p. 140°-5°.

後処理

  1. waitAfter 1 hour
  2. temperaturethe solution was warmed to 100° for 80 minutes
  3. customAfter 18 hours the solution was subjected to evaporation in vacuo
  4. customto give an oil which
  5. customslowly crystallised
  6. customThe solid was recrystallised from EtOH

出典と根拠

ORDレコード
ord-3fe7cfe342a242d3a439e166c0fd66f1
出典データセット
uspto-grants-1987_07
特許番号
US04678794

反応ノート

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